EP1768937B1 - Produits de type gateau humide, a teneur elevee en solides et a tres faibles residus, et procedes de fabrication de ces produits - Google Patents

Produits de type gateau humide, a teneur elevee en solides et a tres faibles residus, et procedes de fabrication de ces produits Download PDF

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Publication number
EP1768937B1
EP1768937B1 EP05706130A EP05706130A EP1768937B1 EP 1768937 B1 EP1768937 B1 EP 1768937B1 EP 05706130 A EP05706130 A EP 05706130A EP 05706130 A EP05706130 A EP 05706130A EP 1768937 B1 EP1768937 B1 EP 1768937B1
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Prior art keywords
kaolin
wet cake
less
ppm
slurry
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German (de)
English (en)
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EP1768937A1 (fr
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Edward J. Sare
James Stacey Johnson
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Imerys Kaolin Inc
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Imerys Kaolin Inc
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Definitions

  • the present invention relates to novel mineral compositions, such as kaolins, having low residue, methods for making such compositions, and their uses, such as the manufacture of top size-sensitive applications, such as ceramic honeycomb automotive substrates, polymers, and rubbers.
  • novel mineral compositions such as kaolins, having low residue
  • methods for making such compositions and their uses, such as the manufacture of top size-sensitive applications, such as ceramic honeycomb automotive substrates, polymers, and rubbers.
  • top size-sensitive applications such as ceramic honeycomb automotive substrates, polymers, and rubbers.
  • Kaolin is a white industrial mineral, which has found use in a wide range of applications. Large deposits of kaolin clay exist in Devon and Cornwall, England, Brazil, China, Australia and in the states of Georgia and South Carolina, United States of America.
  • Particulate kaolins occur naturally in the hydrous form and exist as crystalline structures containing hydroxyl functionality. Particulate kaolins may be converted to a calcined form by thermal processes. Such processes cause the particulate kaolin to dehydroxylate. During calcination, the hydrous kaolin converts from a crystalline to an amorphous form. Further, during calcination, aggregation typically occurs.
  • Hydrous kaolins that can be used in the present invention can be obtained naturally from various locations, such as from the Rio Capim area of Brazil and Georgia of the United States
  • the properties of both hydrous and calcined kaolin are dependent on attributes, such as particle size (expressed in terms of particle size distribution, or PSD), shape, and texture of the individual particles and of agglomerates thereof.
  • particle size expressed in terms of particle size distribution, or PSD
  • shape expressed in terms of shape, and texture of the individual particles and of agglomerates thereof.
  • Calcined kaolin refers to a kaolin that has been converted from the corresponding (naturally occurring) hydrous kaolin to the dehydroxylated form by thermal methods. Calcination changes, among other properties, the kaolin structure from crystalline to amorphous. Calcination is effected by heat-treating coarse or fine hydrous kaolin in known manner, e.g., at temperatures ranging from 500°C to 1200°C, such as temperatures ranging from 800°C to 1200°C.
  • the degree to which hydrous kaolin undergoes changes in crystalline form can depend upon the amount of heat to which the hydrous kaolin is subjected. Initially, dehydroxylation of the hydrous kaolin can occur upon exposure to heat. At temperatures below a maximum of about 850 - 900°C, the product is often considered to be virtually dehydroxylated, with the resultant amorphous structure commonly referred to as a metakaolin. Frequently, calcination at this temperature is referred to "partial calcination,” and the product may also be referred to as “partially calcined kaolin.” Further heating to temperatures above about 900 - 950°C can result in further structural changes, such as densification. Calcination at these higher temperatures is commonly referred to as “full calcination,” and the product is commonly referred to as 'fully calcined kaolin'.
  • Calcined (or “calcination”), as used in herein, may encompass any degree of calcination, including partial (meta) and/or full and/or flash calcination.
  • Calcined kaolin products typically include a small percentage of oversize particles that can have undesirable effects when used in ceramics and can cause blockage of the die in extrusion processes. These oversize particles will generally be retained on a 44 ⁇ m (325 mesh) screen and are commonly referred to as 44 ⁇ m (+325 mesh) residue (or just “residue” herein).
  • the current method for producing a lower residue product is to process the dry standard material through screens to yield the desired residue results.
  • kaolins for "cleaner” lower residue product for use, for example, in thin-walled catalyst production.
  • kaolin wet cake comprising flocculated kaolin, said wet cake having a solids content of at least 50% and a +44 ⁇ m (+325 mesh) residue content of less than or equal to about 50 ppm, such as 20 ppm, 10 ppm, 5 ppm, 2 ppm, and 1 ppm; wherein the kaolin has been wet screened and dewatered, and has a moisture content of greater than or equal to 10%, such as greater than 15%, or 20% subsequent to wet-screening.
  • the feed and slurry may comprise kaolin chosen from hydrous and calcined kaolin. "Chosen from” or “selected from” as used herein refers to selection of individual components or the combination of two (or more) components.
  • the feed and slurry can comprise hydrous kaolin only, calcined kaolin only, or a mixture of hydrous and calcined kaolins,
  • Another aspect of the present disclosure is a method for producing a ceramic body, comprising: screening a fluid kaolin slurry; flocculating the fluid kaolin slurry; dewatering the flocked kaolin slurry to obtain a kaolin wet cake having a solid content of at least 50% and having a +44 ⁇ m (+325 mesh) residue content of not more than about 50 ppm; and forming the kaolin wet cake into a ceramic body, wherein the kaolin is not dried to a moisture content of less than 10%, less than 15%, or even less than 20%, at any time between screening and forming.
  • the kaolin wet cake has a residue content of less than or equal to about 20 ppm, such as 10 ppm, 5 ppm, 2 ppm, and 1 ppm.
  • the fluid kaolin slurry comprises percent solids ranging from about 25% to about 75% solids, such as about 60%, as measured by a CEM AVC-80 microwave solids tester and standard lab operating procedure.
  • the CEM microwave solids tester is a combination microwave oven and four-place analytical balance controlled by an integrated computer.
  • Manufacturer supplied glass fiber pads are the vehicles used to introduce and contain the samples to be tested. Two glass fiber pads are placed on the balance tripod inside the microwave chamber, and the balance is zeroed using the "tare" function key. The pads are then removed and about two grams (total) of sample are placed directly on the pads using transfer pipettes. The pads (containing the sample) are then placed back on the tripod inside the microwave chamber and the machine is started using the "test" function key. The instrument then starts a drying cycle and internally calculates the percent solids of the sample using the weight differential. The results (percent solids) are shown on the display screen.
  • the particle size distribution of a kaolin slurry may be determined by measuring the sedimentation speeds of the dispersed particles of the articulate product under test through a standard dilute aqueous suspension using a SEDIGRAPHTM, e.g., SEDIGRAPH 5100, obtained from Micromeritics Corporation, USA.
  • the size of a given particle can be expressed in terms of the diameter of a sphere of equivalent diameter (esd), which sediments through the suspension.
  • the SEDIGRAPH graphically records the percentage by weight of particles having an esd less than a particular esd value, versus that esd value.
  • Mean particle diameter is defined as the diameter of a circle that has the same area as the largest face of the particle.
  • the mean particle size, d 50 value, and other particle size properties referred to in the present application are measured in a well known manner by sedimentation of the particulate material in a fully dispersed condition in an aqueous medium using a SEDIGRAPH 5100.
  • the mean particle size d 50 is the value determined in this way of the particle esd at which there are 50% by weight of the particles, which have an esd less than that d 50 value.
  • Another aspect provides a fluid kaolin slurry having a particle size distribution of:
  • the slurry undergoes a screening process prior to flocculation.
  • the screening process comprises passing the slurry through a 44 ⁇ m (325 mesh) screen or finer screen.
  • the screening process comprises passing the slurry through a 37 ⁇ m (400 mesh) screen or finer screen, such as a 25 ⁇ m (600 mesh) screen or finer.
  • the kaolin slurry to be screened can be prepared by blunging crude or processed kaolin clay with water to form an aqueous suspension.
  • the slurry further comprises at least one dispersant.
  • the at least one dispersant can be present in an amount effective to fluidize the slurry, for example in an amount ranging from about 0.01% to about 2% by weight, relative to the total weight of the slurry, such as an amount ranging from about 0.01% to about 1% by weight.
  • a dispersing agent is added to the slurry before flocculation, resulting in a pH that is greater than or equal to about 6.5, such as a pH ranging from 8 to 10.
  • the composition can further comprise at least one water-soluble pH modifier.
  • suitable pH-modifiers include sodium carbonate, ammonium carbonate, amino-2-methyl-1-propanol, sodium silicate, sodium hydroxide, and ammonium hydroxide.
  • Dispersants may also be chosen from art recognized organic polymeric dispersants that are traditionally used in kaolin-containing compositions. Appropriate dispersants will be readily apparent to the skilled artisan.
  • dispersants may be chosen from polyelectrolytes such as polyacrylates and copolymers comprising polyacrylate species, for example polyacrylate salts (such as sodium, ammonium and potassium salts), sodium hexametaphosphates, polyphosphoric acid, condensed sodium phosphate, alkanolamines, and other reagents commonly used for this function.
  • Suitable dispersants include 2-amino-2-methyl-1-propanol, tetrasodium pyrophosphate, trisodium phosphate, tetrasodium phosphate, sodium tripolyphosphate, sodium silicate, sodium carbonate, sodium or potassium salts of weak acids, such as condensed naphthalene sulfonic acid and polymeric carboxylic acid, and water-soluble organic polymeric salts, such as sodium or ammonium polyacrylate, and polymethacrylates such as sodium or ammonium polymethacrylate.
  • weak acids such as condensed naphthalene sulfonic acid and polymeric carboxylic acid
  • water-soluble organic polymeric salts such as sodium or ammonium polyacrylate, and polymethacrylates such as sodium or ammonium polymethacrylate.
  • the kaolin wet cake, formed as disclosed herein has a K 2 O content of less than about 2,500 ppm, such as less than about 2000 ppm, less than about 1500 ppm or even less than about 650 ppm.
  • the fluid kaolin slurry is flocculated, typically by lowering the pH of the fluid kaolin slurry to less than or equal to about 5, such as less than or equal to about 4.5.
  • This downward pH adjustment can be accomplished by simply adding an appropriate amount of an acid, such as for example sulfuric acid, alum or other suitable acid.
  • the flocced kaolin slurry may be dewatered in one of the ways well known in the art, e.g. filtration such as via rotary filter or filter press, centrifugation, evaporation and the like, provided that the slurry has a moisture content of greater than or equal to 10%, such as 15% and 20%, at all points between the flocculating and forming processes. Dewatering can also be accomplished with a filter press. Whatever the process, it is understood that wherein the kaolin is not dried to a moisture content of less than 10%, less than 15%, or even less than 20%, at any time between screening and forming.
  • Still further disclosed herein is the use of the kaolin wet cake described above in the formation of cast ceramic ware products.
  • the ceramic composition can comprise a kaolin blend.
  • the kaolin can be blended with other minerals known in the art such as, talc, halloysite, calcium carbonate, titanium dioxide, gypsum, feldspar, nepheline syenite, silica and the like.
  • additional components such as biocides, may be added to the fluid kaolin slurry.
  • Extrusion is a forming method that is commonly used in the production of complex ceramic objects such as the intricate honeycomb ceramics used as substrate supports in automotive catalytic converters.
  • extrusion may be carried out in a number of different ways, such as, for example, the methods disclosed in U.S. Patent No. 3,885,977 to Lachman , U.S. Patent No. 5,332,703 to Hickman et al ., or U.S. Patent No. 5,997,984 to Koike et al .
  • Slip casting is typically used in production of products having complex shapes and where plastic forming or semi-dry pressing are not possible. Thus, slip casting is applicable to the production of, for example, hollow tableware, figures and ornamental ware, and sanitary ware. For whiteware production, 'jiggering' can also be used to produce ware. Slip casting involves the use of a mold of appropriate shape into which a fluid suspension of a body can be poured and wherein the mold progressively extracts some of the water until a solid layer is formed.
  • drain casting Two primary methods are typically employed for slip casting: drain casting and solid casting.
  • drain casting a mold is filled with slip and casting takes place on one surface only. After a suitable time, during which the desired cast thickness is built up, the excess slip is poured off. The mold and cast are then partially dried, to allow mold release, after which the cast can be trimmed, cut or sponged.
  • solid casting which is typically used for products having varying wall thicknesses, the mold is filled with slip and casting takes place on both surfaces. The removal of water generally means that the slip has to be topped up during the casting. For complex shapes, the mold can be constructed in several sections.
  • the method described herein may include a screening process that comprises passing the slurry through a 44 ⁇ m (325 mesh) screen.
  • the +44 ⁇ m (+325 mesh) residue may be measured using standard lab operating procedures. This procedure includes using 100g (dry basis) material in approximately 3,500 ml filtered water to which 60 mls of trisodium polyphosphate (5% strength) have been added.
  • the kaolin sample is then added and mixed vigorously for 20 minutes using a standard lab mixer with good agitation.
  • the material is then poured over a clean 44 ⁇ m (325 mesh) screen, the container is rinsed and this remnant added also.
  • the remaining residue is then washed out into an aluminum pan (weight recorded), and placed under a lamp until completely dry.
  • a simple calculation yields % +325 mesh residue ((sample + pan) - empty pan weight).
  • the method described herein may be applicable to the treatment of other minerals for producing low residue products.
  • Non-limiting examples of such minerals include calcined alumina, tale, aluminum tri-hydrate (ATH), calcium carbonate, dolomite, and silica.
  • percent solids, particle size and % +44 ⁇ m % (+325 mesh) residue were determined on a feed slip.
  • the slip was then screened over a 44 ⁇ m (325 mesh) wire vibrating screen, and the solids, particle size, and % +44 ⁇ m % (+325 mesh) residue were again measured.
  • the sample was then flocced with acid to pH 3.0, and pressed using the Shriver Envirotech filterpress and standard lab operating procedures to yield a cake product with solids around 71%. In some instances, residue measurements were made on the resulting wet cake.
  • Percent solids were measured using the CEM AVC-80 microwave solids tester and standard lab operating procedure as described above.
  • Particle size was determined using the Sedigraph 5100 and standard lab operating procedures, as described above.
  • the Yield (Efficiency) was measured by a simple calculation of - 325 mesh product weight divided by the total feed weight (X100).
  • Example 1 Processed Coarse Samples (Samples 1 and 2)
  • Example 2 shows a processed coarse sample having a median particle size of approximately 8 microns (Sample 1), screened through a 44 ⁇ m (325 mesh) (Sample 2), and the results obtained thereon. This sample was also dried at three various temperatures and the residues only were reevaluated.
  • Example 2 Hydrous Kaolin (Samples 3 and 4)
  • Example 3 Calcined Kaolin (Samples 5, 6, and 7 )

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Claims (37)

  1. Procédé pour produire un corps en céramique, comprenant :
    (a) tamiser une boue fluide de kaolin ;
    (b) floculer la boue fluide de kaolin pour former une boue floculée de kaolin ;
    (c) déshydrater la boue floculée de kaolin pour obtenir un gâteau humide de kaolin avec une teneur en solides d'au moins environ 50% et avec une teneur en résidu +44µm (+325 mesh) inférieure ou égale à 50 ppm ; et
    (d) façonner ledit gâteau humide de kaolin en un corps en céramique ;
    dans lequel ledit kaolin n'est séché à une humidité inférieure à 10% à aucun moment entre les étapes de tamiser et de façonner.
  2. Procédé selon la revendication 1, dans lequel la boue fluide de kaolin a une teneur en solides entre environ 25% et environ 75%.
  3. Procédé selon la revendication 1, dans lequel la boue fluide de kaolin a une teneur en solides d'au moins 60%.
  4. Procédé selon la revendication 1, dans lequel la boue fluide de kaolin est tamisée avec un tamis de 44µm (325 mesh) ou un tamis plus fin.
  5. Procédé selon la revendication 1, dans lequel la boue fluide de kaolin est tamisée avec un tamis de 37µm (400 mesh) ou un tamis plus fin.
  6. Procédé selon la revendication 1, dans lequel la boue fluide de kaolin est tamisée avec un tamis de 25µm (600 mesh) ou un tamis plus fin.
  7. Procédé selon la revendication 1, comprenant en plus disperser la boue fluide de kaolin à l'aide d'un dispersant avant de floculer, où l'étape de disperser se déroule à un pH supérieur à environ 6,5.
  8. Procédé selon la revendication 1, dans lequel le gâteau humide de kaolin a une teneur en K2O inférieure à environ 1500 ppm.
  9. Procédé selon la revendication 1, dans lequel le gâteau humide de kaolin a une teneur en K2O inférieure à environ 650 ppm.
  10. Procédé selon la revendication 1, dans lequel le gâteau humide de kaolin a une teneur en K2O inférieure à environ 20 ppm.
  11. Procédé selon la revendication 1, dans lequel le gâteau humide de kaolin a une teneur en K2O inférieure à environ 10 ppm.
  12. Procédé selon la revendication 1, dans lequel le gâteau humide de kaolin a une teneur en K2O inférieure à environ 5 ppm.
  13. Procédé selon la revendication 1, dans lequel le gâteau humide de kaolin a une teneur en K2O inférieure à environ 2 ppm.
  14. Procédé selon la revendication 1, dans lequel le gâteau humide de kaolin a une teneur en K2O inférieure à environ 1 ppm.
  15. Procédé selon la revendication 1, dans lequel l'étape de floculer comprend réduire le pH de la boue fluide de kaolin à une valeur inférieure ou égale à 5.
  16. Procédé selon la revendication 1, dans lequel le gâteau humide de kaolin est façonné en un corps en céramique par une méthode choisie parmi formage, extrusion, pressage et moulage.
  17. Procédé selon la revendication 1, dans lequel le kaolin comprend du kaolin hydraté.
  18. Procédé selon la revendication 1, dans lequel le kaolin comprend du kaolin calciné.
  19. Procédé selon la revendication 1, dans lequel le gâteau humide de kaolin comprend un mélange de kaolin hydraté et calciné.
  20. Procédé selon la revendication 1, dans lequel ladite boue fluide de kaolin comprend en plus au moins un composant minéral choisi parmi talc, halloysite, carbonate de calcium, gypse, feldspath, silice et syénite néphélinique.
  21. Procédé selon la revendication 1, dans lequel ledit kaolin n'est séché à une humidité inférieure à 15% à aucun moment entre les étapes de tamiser et de façonner.
  22. Procédé selon la revendication 1, dans lequel ledit kaolin n'est séché à une humidité inférieure à 20% à aucun moment entre les étapes de tamiser et de façonner.
  23. Procédé selon la revendication 1, comprenant en plus l'étape d'ajouter un biocide à ladite boue fluide de kaolin.
  24. Gâteau humide de kaolin comprenant du kaolin floculé, ledit gâteau humide ayant une teneur en solides d'au moins 50% et une teneur en résidu +44µm (+325 mesh) inférieure ou égale à 50 ppm ; dans lequel ledit kaolin était tamisé en état humide et déshydraté, et maintenu à une humidité supérieure ou égale à 10% après le tamisage en état humide.
  25. Gâteau humide de kaolin selon la revendication 24 comprenant en plus au moins un composant minéral choisi parmi talc, halloysite, carbonate de calcium, gypse, feldspath, silice et syénite néphélinique.
  26. Gâteau humide de kaolin selon la revendication 24 dans lequel le kaolin comprend du kaolin hydraté.
  27. Gâteau humide de kaolin selon la revendication 24 dans lequel le kaolin comprend du kaolin calciné.
  28. Gâteau humide de kaolin selon la revendication 24 dans lequel la boue fluide de kaolin comprend un mélange de kaolin hydraté et calciné.
  29. Gâteau humide de kaolin selon la revendication 24 dans lequel la teneur en résidu est inférieure ou égale à 20 ppm.
  30. Gâteau humide de kaolin selon la revendication 24 dans lequel la teneur en résidu est inférieure ou égale à 10 ppm.
  31. Gâteau humide de kaolin selon la revendication 24 dans lequel la teneur en résidu est inférieure ou égale à 5 ppm.
  32. Gâteau humide de kaolin selon la revendication 24 dans lequel la teneur en résidu est inférieure ou égale à 2 ppm.
  33. Gâteau humide de kaolin selon la revendication 24 dans lequel la teneur en résidu est inférieure ou égale à 1 ppm.
  34. Usage du gâteau humide de kaolin selon l'une des revendications 24 à 33 dans la production d'un gâteau de filtre en céramique.
  35. Usage du gâteau humide de kaolin selon l'une des revendications 24 à 33 dans la production d'un produit cru.
  36. Usage du gâteau humide de kaolin selon l'une des revendications 24 à 33 dans la production d'un produit de coulage céramique.
  37. Usage du gâteau humide de kaolin selon l'une des revendications 24 à 33 dans la production d'un corps en céramique extrudé.
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